JP2000290013A - Production of alumina particle - Google Patents
Production of alumina particleInfo
- Publication number
- JP2000290013A JP2000290013A JP11100077A JP10007799A JP2000290013A JP 2000290013 A JP2000290013 A JP 2000290013A JP 11100077 A JP11100077 A JP 11100077A JP 10007799 A JP10007799 A JP 10007799A JP 2000290013 A JP2000290013 A JP 2000290013A
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- aluminate
- alumina particles
- aluminum salt
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Cosmetics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はアルミナ粒子特には
板状アルミナ粒子の製造方法に関するものであり、板状
アルミナ粒子にあってはさらに詳しくはアスペクト比が
大きく、粒度分布の狭い粒子表面が滑らかな板状アルミ
ナ粒子を提供し、研磨剤、充填材、化粧料、セラミック
原料、顔料、さらには表面に金属酸化物をコーティング
することにより光輝性顔料としても有用な材料を提供す
るものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing alumina particles, particularly plate-like alumina particles, and more particularly, to a plate-like alumina particle having a large aspect ratio and a narrow particle size distribution. The present invention provides a plate-like alumina particle, and provides an abrasive, a filler, a cosmetic, a ceramic raw material, a pigment, and a material useful as a glitter pigment by coating the surface with a metal oxide.
【０００２】[0002]
【従来の技術】従来、アルミナ粒子特には板状の形態を
有するアルミナ粒子の製造方法としては、特許２６５４
２７６号公報にみられるような水熱処理による方法（以
下水熱合成法）や特開平９−２２７３３７号公報にみら
れるようなフッ素系の鉱化剤の存在下で焼成する方法等
が知られている。2. Description of the Related Art Conventionally, a method for producing alumina particles, particularly, alumina particles having a plate-like form is disclosed in Japanese Patent No. 2654.
A method by hydrothermal treatment (hereinafter referred to as a hydrothermal synthesis method) as disclosed in Japanese Patent Application Laid-Open No. 276/276 and a method of firing in the presence of a fluorine-based mineralizer as disclosed in Japanese Patent Application Laid-Open No. 9-227337 are known. I have.
【０００３】しかし、水熱合成法は、製造方法の観点か
らみて高温反応処理装置を必要とし、設備投資が大掛か
りなものとなり不利であるとともに、製法としても高温
・高圧下での合成であるため、得られる粉体は高価にな
るという問題があった。また、水酸化アルミニウムをハ
ロゲン系のガスの存在下で焼成する方法は、焼成時に発
生するハロゲンガスの処理問題が存在する。さらには酸
性アルミニウム塩に炭酸アルカリ塩を用いて焼成する方
法もあるが、この方法だと中和する時に大量の炭酸が発
生し、扱いにくい問題がある。However, the hydrothermal synthesis method requires a high-temperature reaction apparatus from the viewpoint of the production method, is disadvantageous in that the capital investment becomes large, and the production method is a synthesis under high temperature and high pressure. However, there is a problem that the obtained powder becomes expensive. Further, the method of firing aluminum hydroxide in the presence of a halogen-based gas has a problem of treating halogen gas generated during firing. Further, there is a method of calcining using an acidic aluminum salt with an alkali carbonate, but this method has a problem that a large amount of carbonic acid is generated at the time of neutralization and is difficult to handle.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、このような
従来技術における多くの課題を改善することを目的と
し、凝集のない粒度分布がシャープなアルミナ粒子さら
にはこれらを含み表面が滑らかな板状アルミナ粒子の簡
便な製造方法を提供することを目的とする。SUMMARY OF THE INVENTION It is an object of the present invention to solve many of the problems in the prior art, and it is an object of the present invention to provide an alumina particle having a sharp particle size distribution without agglomeration, and a plate containing these particles having a smooth surface. It is an object of the present invention to provide a simple method for producing alumina particles.
【０００５】[0005]
【課題を解決するための手段】本発明は、下記の構成よ
りなる。The present invention comprises the following constitutions.
【０００６】（１）アルミン酸塩と酸性アルミニウム塩
とを水を含んだ状態で反応させることにより、アルミナ
又は／及びアルミナ水和物と中和金属塩を含む混合物を
製造し、この混合物を１０００〜１６００℃で焼成する
ことを特徴とするアルミナ粒子の製造方法。(1) A mixture containing alumina or / and alumina hydrate and a neutralized metal salt is produced by reacting an aluminate and an acidic aluminum salt in a state containing water, and this mixture is mixed with 1000 parts. A method for producing alumina particles, characterized by firing at 1600 ° C.
【０００７】（２）アルミナ又は／及びアルミナ水和物
が非晶質又は／及び結晶質である上記（１）記載のアル
ミナ粒子の製造方法。 （３）アルミン酸塩と酸性アルミニウム塩と燐酸塩とを
水を含んだ状態で反応させる（１）記載のアルミナ粒子
の製造方法。(2) The method for producing alumina particles according to the above (1), wherein the alumina or / and alumina hydrate is amorphous or / and crystalline. (3) The method for producing alumina particles according to (1), wherein the aluminate, the acidic aluminum salt and the phosphate are reacted in a state containing water.
【０００８】（４）アルミン酸塩にアルカリ性の燐酸塩
を添加したものと酸性アルミニウム塩を混合したものを
水分を含んだ状態で反応させる上記（１）記載のアルミ
ナ粒子の製造方法。 （５）アルミン酸塩と酸性アルミニウム塩に酸性の燐酸
塩を添加したものを水分を含んだ状態で反応させる上記
（１）記載のアルミナ粒子の製造方法。 （６）アルミン酸塩と酸性アルミニウム塩と燐酸塩とを
混合した時の水素イオン濃度がｐＨ＝６〜１０の範囲で
ある上記（３）〜（５）のいずれかに記載のアルミナ粒
子の製造方法。(4) The method for producing alumina particles according to the above (1), wherein a mixture of an aluminate to which an alkaline phosphate is added and a mixture of an acidic aluminum salt are reacted while containing water. (5) The method for producing alumina particles according to the above (1), wherein an aluminate and an acidic aluminum salt to which an acidic phosphate is added are reacted in a state containing water. (6) The production of alumina particles according to any of (3) to (5) above, wherein the hydrogen ion concentration when the aluminate, the acidic aluminum salt and the phosphate are mixed is in the range of pH = 6 to 10. Method.
【０００９】（７）平均粒子径が０．２〜１００μｍ、
厚みが３μｍ以下、アスペクト比（粒子径／厚み）が５
以上である板状アルミナ粒子を製造する上記（３）〜
（６）のいずれかに記載のアルミナ粒子の製造方法。(7) an average particle diameter of 0.2 to 100 μm;
Thickness of 3 μm or less, aspect ratio (particle diameter / thickness) of 5
The above (3) to above for producing plate-like alumina particles as described above
The method for producing alumina particles according to any one of (6).
【００１０】本発明において用いられるアルミン酸塩は
水酸化アルカリの溶液にアルミニウム又は水酸化アルミ
ニウムを溶かしたものであれば何でもよく、例えばＮａ
ＡｌＯ2、ＫＡｌＯ2のようなＭＡｌＯ2（Ｍは一価の金
属）の構造式をとるアルカリ金属塩やＮａＡｌＯ2・５
／４Ｈ2Ｏ、ＮａＡｌＯ2・３Ｈ2Ｏ、ＫＡｌＯ2・３／２
Ｈ2ＯのようなＭＡｌＯ2・ｎＨ2Ｏ（Ｍは一価の金属）
の構造式をとるもの、更には一般式でｘＭ2Ｏ・ｙＡｌ2
Ｏ3・ｚＨ2Ｏ（Ｍは一価の金属、ｚ＝０を含む）の構造
式をとるものである。又、酸性アルミニウム塩は、酸性
溶液にアルミニウム又は水酸化アルミニウムを溶かした
ものであれば何でもよく、酸性溶液としては例えば燐酸
や硫酸のような鉱酸または蓚酸やマレイン酸、マロン酸
のような有機酸が挙げられる。具体的には硫酸アルミニ
ウム、塩化アルミニウムなどがある。The aluminate used in the present invention may be any one obtained by dissolving aluminum or aluminum hydroxide in an alkali hydroxide solution.
An alkali metal salt having a structural formula of MAlO 2 (M is a monovalent metal) such as AlO 2 or KAlO 2 or NaAlO 2 .5
/ 4H 2 O, NaAlO 2 · 3H 2 O, KAlO 2 · 3/2
MAlO 2 .nH 2 O such as H 2 O (M is a monovalent metal)
And the general formula xM 2 O.yAl 2
It has a structural formula of O 3 .zH 2 O (M is a monovalent metal, including z = 0). The acidic aluminum salt may be any solution in which aluminum or aluminum hydroxide is dissolved in an acidic solution. Examples of the acidic solution include mineral acids such as phosphoric acid and sulfuric acid and organic acids such as oxalic acid, maleic acid and malonic acid. Acids. Specific examples include aluminum sulfate and aluminum chloride.
【００１１】又、燐酸塩は結晶成長剤としての作用があ
り、板状アルミナを作製する上では必要であり、燐酸、
燐酸ソーダ、燐酸カリ、燐酸アンモニウム、ピロ燐酸ソ
ーダ、ピロ燐酸カリ、トリポリ燐酸ソーダ、トリポリ燐
酸アンモニウムなどが挙げることができる。この燐酸塩
の添加量は、アルミナに換算して０．０１重量％以上で
あることが好ましい。アルミン酸塩に酸性アルミニウム
塩又はこれに燐酸塩を混合した水溶液を混合し、加水分
解生成物と中和塩を含む懸濁液またはゲルとする。中和
塩は焼成時において、溶融状態となり、このときアルミ
ナ化及びアルミナの板状化を促進する効果があり、中和
の量はアルミナ重量１に対して０．１〜７倍が好まし
い。０．１倍未満ではアルミナ化及びアルミナの板状化
に十分な効果を発揮せず、また７倍を超えると洗浄時に
相当な負担がかかるためである。Phosphate acts as a crystal growth agent and is necessary for producing plate-like alumina.
Examples include sodium phosphate, potassium phosphate, ammonium phosphate, sodium pyrophosphate, potassium pyrophosphate, sodium tripolyphosphate, and ammonium tripolyphosphate. The amount of the phosphate is preferably 0.01% by weight or more in terms of alumina. The aluminum salt is mixed with an acidic aluminum salt or an aqueous solution obtained by mixing a phosphate with the aluminum salt to form a suspension or gel containing a hydrolysis product and a neutralization salt. The neutralized salt is in a molten state at the time of firing, and has an effect of promoting aluminization and plate formation of alumina. The amount of neutralization is preferably 0.1 to 7 times the weight of alumina. If the ratio is less than 0.1 times, sufficient effect for alumina conversion and plate formation of alumina is not exerted, and if the ratio exceeds 7 times, a considerable load is imposed upon cleaning.
【００１２】その後乾燥粉末を１０００〜１６００℃で
焼成する焼成温度が１０００℃未満であるとアルミナ化
（特には板状アルミナ化）するまでに長時間を要し、経
済的ではなく、又、１６００℃を越えるとアルミナ（特
には板状アルミナ）の粒子同士が焼結をしてしまうため
である。このような焼結をより確実に防ぐためには、焼
成温度を１４００℃以下とすることがより好ましい。If the firing temperature at which the dried powder is fired at 1000 to 1600 ° C. is lower than 1000 ° C., it takes a long time to aluminize (particularly plate-like alumina), which is not economical. If the temperature exceeds ℃, alumina (particularly, plate-like alumina) particles are sintered. In order to more reliably prevent such sintering, the firing temperature is more preferably set to 1400 ° C. or lower.
【００１３】水素イオン濃度をｐＨ６〜１０の範囲にし
た場合、アルミナ水和物の析出が効率的になされ、アル
ミナ（特には板状アルミナ）を効率良く製造することが
できる。非晶質アルミナ又は／及び結晶質アルミナ粒子
と中和金属塩との混合物は、焼成後に生成される粒子同
士の凝集を防ぐため、焼成前に蒸散乾燥し、その後、混
合物を解することが好ましい。又、焼成後においては、
熔融塩処理し固形分を得た後、この固形分を水洗し、濾
取し乾燥することが好ましい。When the hydrogen ion concentration is in the range of pH 6 to 10, alumina hydrate is efficiently precipitated, and alumina (particularly, plate-like alumina) can be efficiently produced. The mixture of the amorphous alumina and / or crystalline alumina particles and the neutralized metal salt is preferably evaporated and dried before firing, and then the mixture is disintegrated, in order to prevent aggregation of the particles generated after firing. . Also, after firing,
After obtaining a solid content by performing a molten salt treatment, it is preferable that the solid content be washed with water, collected by filtration, and dried.
【００１４】このようにして得られた本発明に係るアル
ミナ粒子の場合、平均粒子径の０．２〜１００μｍの粒
状アルミナ粒子であり、特に板状アルミナ粒子はＳＥＭ
観察の結果、大きな平均粒子径で０．２〜１００μｍ、
厚みが３μｍ以下アスペクト比（粒子径／厚み）が５以
上である板状アルミナ粒子であり、水に対して分散し撹
拌したところ、流線（偏平粒子を液中に懸濁させ撹拌さ
せた際に分散性が良いと粒子の一連の流れが粒子表面の
反射光が層状の縞模様となって観察される現象）がみら
れ、分散性が極めて良好なものであった。板状アルミナ
粒子を分析した結果、リン及びリン化合物や中和塩が検
出されず、洗浄工程において除去されているものと考え
られる。The alumina particles according to the present invention thus obtained are granular alumina particles having an average particle diameter of 0.2 to 100 μm, and particularly, plate-like alumina particles are SEM.
As a result of the observation, a large average particle diameter of 0.2 to 100 μm,
A plate-like alumina particle having a thickness of 3 μm or less and an aspect ratio (particle diameter / thickness) of 5 or more. When dispersed and stirred in water, streamline (when flat particles are suspended in a liquid and stirred) When the dispersibility is good, a phenomenon in which a series of flow of particles is observed as reflected light on the particle surface as a layered stripe pattern) was observed, and the dispersibility was extremely good. As a result of analyzing the plate-like alumina particles, it is considered that phosphorus, the phosphorus compound, and the neutralized salt were not detected, and were removed in the washing step.
【００１５】本発明に係るアルミナ粒子及び板状アルミ
ナ粒子はそのままセラミックスの原料とすることがで
き、あるいは塗料用、プラスチック等の充填剤、化粧料
用、研磨剤、釉薬用等の顔料として優れているものであ
る。特に板状アルミナ粒子の場合、前述の用途に有用で
あり、さらに金属酸化物をコーティングすることによっ
て光輝性顔料としての有用性はさらに増す。The alumina particles and plate-like alumina particles according to the present invention can be used as raw materials for ceramics as they are, or they are excellent as pigments for paints, fillers such as plastics, cosmetics, abrasives, glazes and the like. Is what it is. In particular, in the case of plate-like alumina particles, they are useful for the above-mentioned applications. Further, by coating a metal oxide, the usefulness as a glitter pigment is further increased.
【００１６】[0016]
【発明の実施の形態】次に実施例により本発明を更に詳
細に説明するが、本発明はこれらの実施例に限定される
ものではない。Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００１７】実施例１ 水酸化ナトリウム２０ｇを水中で溶液とし、この溶液に
金属アルミニウム５ｇ及び燐酸水素２ナトリウム０．２
５ｇ入れ溶液中に撹拌しながら溶かす。その後この混合
溶液中に硫酸アルミニウム水溶液をｐＨ＝７になるまで
撹拌しながら投入する。混合したものは白濁状のゲルと
なり、これをそのまま蒸散乾燥した。この時の蒸散乾燥
した固形分のＸ線回折の結果、結晶質のものとして硫酸
ナトリウムが同定された。その後１２００℃で５時間保
持の条件で焼成した。得られた処理物に水を加え洗浄、
濾過し、固形分を乾燥し板状アルミナ粉体を得た。得ら
れた板状アルミナをＸ線回折法により生成物を同定した
ところ、酸化アルミニウム（αアルミナ）であった。Ｓ
ＥＭにて観察してみたところ板状粒子であり、粒度分布
計で粒度を測定したところ中心粒径が１０μｍであり、
シャープな分布となっていた。又、この粉末を水に混ぜ
てみたところ、きれいな流紋が確認された。 実施例２ 水酸化ナトリウム２０ｇを６０℃の水中で溶液とし、こ
の溶液に金属アルミニウム５ｇ及び燐酸水素２ナトリウ
ム０．２５ｇ入れ溶液中に撹拌しながら溶かす。その後
この混合溶液中に６０℃の硫酸アルミニウム水溶液をｐ
Ｈ＝９になるまで撹拌しながら投入する。混合したもの
は白濁状のゲルとなり、そのまま更に６０分撹拌した
後、蒸散乾燥した。この時の蒸散乾燥した固形分のＸ線
回折の結果、擬ベーマイトである事を確認した。蒸散乾
燥した固形分を１２００℃で５時間保持の条件で焼成し
た。得られた処理物に水を加え洗浄、濾過し、固形分を
乾燥し板状アルミナ粉体を得た。得られた板状アルミナ
をＸ線回折法により生成物を同定したところ、酸化アル
ミニウム（αアルミナ）であった。ＳＥＭにて観察して
みたところ板状粒子であり、粒度分布計で粒度を測定し
たところ中心粒径が１０μｍであり、シャープな分布と
なっていた。又、この粉末を水に混ぜてみたところ、き
れいな流紋が確認された。Example 1 A solution of 20 g of sodium hydroxide in water was added to 5 g of metallic aluminum and 0.2 g of disodium hydrogen phosphate.
Add 5 g and dissolve into the solution with stirring. Thereafter, an aqueous solution of aluminum sulfate is introduced into the mixed solution with stirring until the pH becomes 7. The resulting mixture turned into a cloudy gel, which was evaporated and dried as it was. As a result of X-ray diffraction of the evaporated and dried solid, sodium sulfate was identified as a crystalline substance. Then, it was baked at 1200 ° C. for 5 hours. Water is added to the obtained processed material and washed,
After filtration, the solid content was dried to obtain a plate-like alumina powder. When the product of the obtained plate-like alumina was identified by an X-ray diffraction method, it was found to be aluminum oxide (α-alumina). S
When observed with EM, it was plate-like particles, and the particle size was measured with a particle size distribution analyzer, and the central particle size was 10 μm.
It had a sharp distribution. Further, when this powder was mixed with water, a clean ripple was confirmed. Example 2 20 g of sodium hydroxide was made into a solution in water at 60 ° C., and 5 g of metallic aluminum and 0.25 g of disodium hydrogen phosphate were put into this solution and dissolved in the solution with stirring. Thereafter, an aqueous solution of aluminum sulfate at 60 ° C.
Charge with stirring until H = 9. The resulting mixture became a cloudy gel, and the mixture was further stirred for 60 minutes and then evaporated to dryness. As a result of X-ray diffraction of the evaporated and dried solid, it was confirmed to be pseudo-boehmite. The evaporated and dried solid was fired at 1200 ° C. for 5 hours. Water was added to the obtained treated product, which was washed, filtered, and the solid content was dried to obtain a plate-like alumina powder. When the product of the obtained plate-like alumina was identified by an X-ray diffraction method, it was found to be aluminum oxide (α-alumina). Observation with an SEM revealed that the particles were plate-like particles, and the particle size was measured with a particle size distribution meter. The central particle size was 10 μm, and the distribution was sharp. Further, when this powder was mixed with water, a clean ripple was confirmed.
【００１８】実施例３ アルミン酸ナトリウム２０ｇを６０℃の水に溶解させ、
その中に硫酸アルミニウム水溶液を加えｐＨ＝９になる
ように調整し、そのまま６０分撹拌した。その後蒸散乾
燥させ、乾燥した固形分のＸ線回折の結果、擬ベーマイ
トの回折ピークが確認された。この乾燥固形分を１２０
０℃、５時間焼成し、洗浄、濾過し、固形分を乾燥し
た。得られた物をＸ線回折により同定した結果、酸化ア
ルミナ（αアルミナ）であった。ＳＥＭにて観察してみ
たところ、０．２μｍの粒状であり、板状粒子ではなか
った。又、この粉末を水に混ぜてみたところ、流紋が確
認されなかった。Example 3 20 g of sodium aluminate was dissolved in water at 60 ° C.
An aqueous solution of aluminum sulfate was added thereto to adjust the pH to 9, and the mixture was stirred for 60 minutes. Thereafter, it was evaporated and dried, and as a result of X-ray diffraction of the dried solid, a diffraction peak of pseudo-boehmite was confirmed. This dry solid content is 120
The mixture was baked at 0 ° C. for 5 hours, washed, filtered, and the solid content was dried. As a result of identifying the obtained product by X-ray diffraction, it was found to be alumina oxide (α-alumina). Observation with an SEM revealed that the particles were 0.2 μm in particle size and not plate-like particles. Further, when this powder was mixed with water, no ripple was observed.
【００１９】[0019]
【発明の効果】本発明によれば凝集のない独立し、かつ
粒度分布がシャープなアルミナ粒子が特に高圧を必要と
することなく容易に得られる。特に燐酸塩を用いた場合
には板状アルミナ粒子が生成する。またハロゲン系の鉱
化剤を使用しないため、作業環境を汚染することがな
い。According to the present invention, alumina particles free of aggregation and having a sharp particle size distribution can be easily obtained without particularly requiring a high pressure. In particular, when a phosphate is used, plate-like alumina particles are generated. Further, since no halogen-based mineralizer is used, the working environment is not polluted.
Claims (7)
水を含んだ状態で反応させることにより、アルミナ又は
／及びアルミナ水和物と中和金属塩を含む混合物を製造
し、この混合物を１０００〜１６００℃で焼成すること
を特徴とするアルミナ粒子の製造方法。A mixture containing alumina and / or hydrated alumina and a neutralized metal salt is produced by reacting an aluminate and an acidic aluminum salt in a state containing water. A method for producing alumina particles, characterized by firing at 1600 ° C.
晶質又は／及び結晶質である請求項１記載のアルミナ粒
子の製造方法。2. The method for producing alumina particles according to claim 1, wherein the alumina and / or alumina hydrate is amorphous or / and crystalline.
酸塩とを水を含んだ状態で反応させる請求項１記載のア
ルミナ粒子の製造方法。3. The method for producing alumina particles according to claim 1, wherein the aluminate, the acidic aluminum salt and the phosphate are reacted in a state containing water.
加したものと酸性アルミニウム塩を混合したものを水分
を含んだ状態で反応させる請求項１記載のアルミナ粒子
の製造方法。4. The process for producing alumina particles according to claim 1, wherein a mixture of an aluminate and an alkaline aluminum phosphate and a mixture of an acidic aluminum salt are reacted in a state containing water.
性の燐酸塩を添加したものを水分を含んだ状態で反応さ
せる請求項１記載のアルミナ粒子の製造方法。5. The process for producing alumina particles according to claim 1, wherein an aluminate and an acidic aluminum salt to which an acidic phosphate is added are reacted in a state containing water.
酸塩とを混合した時の水素イオン濃度がｐＨ＝６〜１０
の範囲である請求項３〜５のいずれかに記載のアルミナ
粒子の製造方法。6. A mixture of an aluminate, an acidic aluminum salt and a phosphate, having a hydrogen ion concentration of pH = 6-10.
The method for producing alumina particles according to any one of claims 3 to 5, wherein
が３μｍ以下、アスペクト比（粒子径／厚み）が５以上
である板状アルミナ粒子を製造する請求項３〜６のいず
れかに記載のアルミナ粒子の製造方法。7. A plate-like alumina particle having an average particle diameter of 0.2 to 100 μm, a thickness of 3 μm or less, and an aspect ratio (particle diameter / thickness) of 5 or more is produced. A method for producing alumina particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10007799A JP3711318B2 (en) | 1999-04-07 | 1999-04-07 | Method for producing alumina particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10007799A JP3711318B2 (en) | 1999-04-07 | 1999-04-07 | Method for producing alumina particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000290013A true JP2000290013A (en) | 2000-10-17 |
| JP3711318B2 JP3711318B2 (en) | 2005-11-02 |
Family
ID=14264394
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10007799A Expired - Lifetime JP3711318B2 (en) | 1999-04-07 | 1999-04-07 | Method for producing alumina particles |
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| Country | Link |
|---|---|
| JP (1) | JP3711318B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002235026A (en) * | 2001-02-09 | 2002-08-23 | Sakura Color Prod Corp | Solid drawing material |
| JP2003073603A (en) * | 2001-08-30 | 2003-03-12 | Sakura Color Prod Corp | Ink composition for water ink ball-point pen, and ball- point pen using the same |
| JP2004155630A (en) * | 2002-11-08 | 2004-06-03 | Showa Denko Kk | Alumina particle and method of manufacturing the same |
-
1999
- 1999-04-07 JP JP10007799A patent/JP3711318B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002235026A (en) * | 2001-02-09 | 2002-08-23 | Sakura Color Prod Corp | Solid drawing material |
| JP4712200B2 (en) * | 2001-02-09 | 2011-06-29 | 株式会社サクラクレパス | Solid drawing material |
| JP2003073603A (en) * | 2001-08-30 | 2003-03-12 | Sakura Color Prod Corp | Ink composition for water ink ball-point pen, and ball- point pen using the same |
| JP2004155630A (en) * | 2002-11-08 | 2004-06-03 | Showa Denko Kk | Alumina particle and method of manufacturing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3711318B2 (en) | 2005-11-02 |
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